反応 #7644

反応方程式

2-aminobutanoic acid

chlorotrimethylsilane

cyclopentanecarbonyl chloride

triethylamine

→

2-[(Cyclopentylcarbonyl)amino]butanoic acid

溶媒

dichloromethane

water

water

dichloromethane

反応条件

後処理

1. 1
   workup.STIRRINGthe mixture is stirred for 1 hour at room temperature and 1 hour at 40° C
2. 2
   温度After cooling down at −10° C.
3. 3
   workup.STIRRINGThe reaction mixture is stirred for 2 hours at −10° C.
4. 4
   その他1 hour
5. 5
   その他at room temperature
6. 6
   ろ過filtered
7. 7
   洗浄the solid product washed with water/dichloromethane 9/1, toluene and diethylether

実験手順

35 g (339 mmol) 2-aminobutanoic acid and 75.6 g (747 mmol) triethylamine are suspended in 300 ml of dichloromethane and stirred at 0° C. 81 g (747 mmol) chlorotrimethylsilane are added dropwise, then the mixture is stirred for 1 hour at room temperature and 1 hour at 40° C. After cooling down at −10° C., 45 g (339 mmol) cyclopentanecarbonyl chloride are added slowly. The reaction mixture is stirred for 2 hours at −10° C. and then 1 hour at room temperature. At 0° C., 50 ml of water are added. The mixture is diluted with water and dichloromethane, filtered and the solid product washed with water/dichloromethane 9/1, toluene and diethylether.

出典